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建立了气相色谱-质谱法检测牛初乳中β-雌二醇质量浓度的方法。牛初乳经过β-葡萄糖醛酸酶/芳香基硫酸酯酶水解后,经过乙腈超声提取、沉淀蛋白,正己烷去除脂肪,HLB固相萃取柱富集净化后,氮气流下吹干,N,O-双(三甲基硅烷基)三氟乙酰胺(BSTFA)衍生,N-甲基-N-三甲基硅基三氟乙酰胺(TMCS)辅助催化,气相色谱-质谱(GC-MS)对衍生物进行检测分析。β-雌二醇质量浓度在5~200μg/L之间线性关系良好,相关系数(R2)大于0.999;加标回收率在85.13%~104.78%之间,相对标准偏差在4.74%~5.97%之间。该方法操作简便、灵敏,精密度好,适用于牛初乳中β-雌二醇的测定。
A method for the determination of β-estradiol in colostrum by gas chromatography-mass spectrometry was established. Bovine colostrum is hydrolyzed by β-glucuronidase / aryl sulfatase, and then is subjected to ultrasonic extraction with acetonitrile to precipitate protein and n-hexane to remove fat. HLB solid-phase extraction column is enriched and purified, dried under nitrogen flow, and N, O (Trimethylsilyl) trifluoroacetamide (BSTFA) derivatization, assisted by N-methyl-N-trimethylsilyl trifluoroacetamide (TMCS) and gas chromatography-mass spectrometry Derivatives for testing and analysis. The linearity of β-estradiol was in the range of 5 ~ 200 μg / L with the correlation coefficient (R2) greater than 0.999. The recoveries of standard addition ranged from 85.13% to 104.78% with relative standard deviations between 4.74% and 5.97% between. The method is simple, sensitive and precise, and is suitable for the determination of β-estradiol in colostrum.